CN108395562A - A kind of preparation method of high-crystallinity bacteria cellulose powder - Google Patents
A kind of preparation method of high-crystallinity bacteria cellulose powder Download PDFInfo
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- CN108395562A CN108395562A CN201810540772.2A CN201810540772A CN108395562A CN 108395562 A CN108395562 A CN 108395562A CN 201810540772 A CN201810540772 A CN 201810540772A CN 108395562 A CN108395562 A CN 108395562A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/14—Chemical modification with acids, their salts or anhydrides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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Abstract
The invention discloses a kind of preparation methods of high-crystallinity bacteria cellulose powder, by fermentation prepare and bacteria cellulose film after purification by oxalic acid dipping, heated-air drying, grinding, remove oxalic acid, membranaceous BC is become powdered, and the property that ethyl alcohol is soluble in using oxalic acid is easily removed oxalic acid, this method is easy to operate, it is at low cost, and obtained BC powder has very high crystallinity, it can be widely applied for packaging material for food, the fields such as artificial skin, beauty, paper industry obtain preferable market prospects and interests.
Description
【Technical field】
The invention belongs to the preparation method of bacteria cellulose powder, more particularly to a kind of high-crystallinity bacteria cellulose powder
Preparation method.
【Background technology】
Bacteria cellulose (Bacteria Cellulose, abbreviation BC) is one kind by acetobacter xylinum (Acetobacter
The general name of the cellulose of microbial fermentations synthesis such as xylinum).Compared with plant cellulose, BC has high-purity, high water holding
The features such as property, high-tensile, good biocompatibility, it is therefore widely used in biological medicine, food, cosmetics, spinning
Many fields such as weaver's industry, molecular filter.
In paper industry, often BC is added in paper pulp to prepare the paper that wet strength is high, dry strength is high, durability is good.
And BC has nanoscale three-dimensional reticular structure, fiber size is very small, can be directly strong bonded with polymer matrix.Than plant fibre
Dimension element has more advantage, and BC makees reinforcing material and polymer appropriate is compound, can prepare with specific use or high performance life
Object based composites.
Currently marketed bacterial cellulose product is occurred with gel form, function and limited efficacy, is also not easy to grow
Phase preservation is bulky simultaneously, transports and inconvenient to carry, application can be widened by being made into powder.But BC has hyperfine three
Reticular structure is tieed up, intermolecular force is very strong, it is difficult to powder be made, difficulty is brought with production to processing.Nowadays with spraying
Though a variety of drying modes such as dry can prepare bacteria cellulose powder but manufactured powder size is inhomogenous, many excellent spies
Property lose, and cost is excessively high, is not suitable for industrial production.
Therefore a kind of simple method for preparing bacteria cellulose powder of research invention can widen BC applications.
【Invention content】
The purpose of the present invention is to provide a kind of preparation method of high-crystallinity bacteria cellulose powder, this method is simply easy
Row can effectively solve the problem that bacteria cellulose powder hardly possible and edible safety problem, widen the application range of BC.
The present invention uses following technical scheme：
A kind of preparation method of high-crystallinity bacteria cellulose powder, is immersed in quality percentage by bacteria cellulose film first
In the oxalic acid solution that specific concentration is 1%~20%, bacteria cellulose film is then taken out, its surface moisture is blotted, is then done
It is dry to constant weight, be finally ground to it is powdered, obtain bacteria cellulose powder.
After bacteria cellulose is immersed in oxalic acid solution, impregnated using ultrasonic wave assistant soakage or water-bath.
Use the condition of ultrasonic wave assistant soakage for：90~100W of power, temperature be 50~60 DEG C, the time be 15~
30min；Use water-bath impregnate condition for：Temperature is 80~90 DEG C, 1~2h of time.
The bacteria cellulose film is so that corn gluten water culture medium is left to ferment and is obtained, and standing for fermentation is specially temperature
28~32 DEG C, the time：6~10 days.
The corn gluten water culture medium ingredient is：Maize pulp-water thinner ratio 1:4, sucrose 33.2g/L, calcium chloride
23g/L, KH2PO41.2g/L, MgSO40.5g/L, ethyl alcohol 16.2ml/L, the culture medium are acid solution.
The bacteria cellulose film is immersed in alkaline solution first before being immersed in oxalic acid solution, is boiled
To remove remaining thalline and culture medium, until bacteria cellulose film be creamy white it is translucent.
The bacteria cellulose film should remove surface impurity first, then remove residual thalline and culture medium, last more
Secondary flushing is neutrality up to solution, is finally immersed in distilled water and refrigerates.
The bacteria cellulose film a diameter of 8 ± 0.30cm, thickness 6mm~10mm.
The bacteria cellulose film is ground after powder, absolute ethyl alcohol to be added, waits for that ethyl alcohol volatilizees naturally.
Compared with prior art, the present invention has technique effect beneficial below：
The preparation method of high-crystallinity bacteria cellulose powder disclosed by the invention is will to ferment to prepare and after purification thin
Membranaceous BC is become powdered, and utilize by fungin film by oxalic acid dipping, heated-air drying, grinding, removing oxalic acid
The property that oxalic acid is soluble in ethyl alcohol easily removes oxalic acid, and this method is easy to operate, at low cost, and obtained BC powder has very
High crystallinity (crystallinity 30~42%), can be widely applied for packaging material for food, artificial skin, beauty, paper industry
Equal fields, obtain preferable market prospects and interests.
【Description of the drawings】
Fig. 1 is the X diffraction patterns of the BC powder prepared through the method for the present invention.
【Specific implementation mode】
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
The preparation method of high-crystallinity bacteria cellulose powder disclosed by the invention, includes the following steps：
1, the preparation and purification of bacteria cellulose
Corn gluten water culture medium after bacteria cellulose film is optimized by laboratory is left to ferment and obtains, standing for fermentation tool
Body is 28~32 DEG C of temperature, time：6~10 days.Medium component is as follows：Maize pulp-water thinner ratio 1:1~1:5, sucrose
33.2g/L CaCl223g/L, KH2PO41.2g/L, MgSO40.5g/L, ethyl alcohol 16.2ml/L, pH 5.
The purifying of BC：The BC film distilled water flushings for taking out fermentation are multiple, after surface impurity is removed, then immerse 0.1~
In the NaOH solution of 0.2mol/L, boil 1~2h to remove remaining thalline and culture medium, until film be creamy white it is translucent
Shape.It is rinsed repeatedly to neutrality, is immersed stored refrigerated for use in distilled water with a concentration of 0.5~1% acetic acid and distilled water afterwards.
2, the powder pre-treatment processed of bacteria cellulose
(1) a piece of bacteria cellulose film (8 ± 0.30cm of diameter, thickness 6mm~10mm) prepared is taken to be respectively put into
In 1%~20% oxalic acid solution.It is respectively adopted:1. taking ultrasonic wave assistant soakage, 90~100W of power, temperature is 50~60
DEG C, the time is 15~30min.2. water-bath is taken to impregnate, temperature is 80~90 DEG C, 1~2h of time.
3, the drying of bacteria cellulose
The bacteria cellulose film that taking-up was impregnated with oxalic acid solution blots surface moisture with filter paper, is placed in preheating 90~120
Middle drying is to constant weight in DEG C electric heating constant-temperature blowing drying box.
4, the preparation of bacteria cellulose powder
Dry bacteria cellulose film is taken out, is put in bowl and is ground into powder.
5, the removal of oxalic acid
Bacteria cellulose powder is placed in 100mL beakers, point 2~3 addition absolute ethyl alcohol washings, residual ethanol is natural
Volatilization.
Bacteria cellulose film after being impregnated by the oxalic acid solution of various concentration only simple grinding can powder processed, and be soaked in water
It is difficult to crush after the drying of BC films, wherein the bacteria cellulose of ultrasonic assistant soakage is easier to be milled than what water-bath impregnated, 10%
BC film brittleness increases after oxalic acid solution impregnates, and is more easy to pulverize, particle is thinner, and crystallinity is higher.
Embodiment 1
1, the preparation and purification of bacteria cellulose
For bacteria cellulose film by laboratory with corn gluten water culture medium is left to ferment and is obtained, standing for fermentation is specially temperature
28~32 DEG C, the time：6~10 days.
The purifying of BC：The BC film distilled water flushings for taking out fermentation are multiple, after surface impurity is removed, then immerse
In the NaOH solution of 0.1mol/L, boil 2h to remove remaining thalline and culture medium, until film be creamy white it is translucent.Afterwards
It is rinsed repeatedly to neutrality, is immersed stored refrigerated for use in distilled water with a concentration of 1% acetic acid and distilled water.
2, the powder pre-treatment processed of bacteria cellulose
The a piece of bacteria cellulose film (8 ± 0.30cm of diameter, thickness 6mm~10mm) prepared is taken to be immersed in a concentration of
In 1% oxalic acid solution.It is 60 DEG C to take ultrasonic wave assistant soakage, power 100W, temperature, time 15min.
3, the drying of bacteria cellulose
The bacteria cellulose film that taking-up was impregnated with oxalic acid solution blots surface moisture with filter paper, is placed in 105 DEG C of electricity of preheating
Middle drying is to constant weight in hot constant temperature blast drying oven.
4, the preparation of bacteria cellulose powder
Dry bacteria cellulose film is taken out, is put in bowl and is ground into powder.
5, the removal of oxalic acid
Bacteria cellulose powder is placed in 100mL beakers, point 2~3 addition absolute ethyl alcohol washings, residual ethanol is natural
Volatilization.
Embodiment 2
1, the preparation and purification of bacteria cellulose
Corn gluten water culture medium is left to ferment and obtains after bacteria cellulose film is optimized by laboratory, and standing for fermentation is specific
For 28~32 DEG C of temperature, time：6~10 days.
The purifying of BC：The BC film distilled water flushings for taking out fermentation are multiple, after surface impurity is removed, then immerse
In the NaOH solution of 0.1mol/L, boil 2h to remove remaining thalline and culture medium, until film be creamy white it is translucent.Afterwards
It is rinsed repeatedly to neutrality, is immersed stored refrigerated for use in distilled water with a concentration of 1% acetic acid and distilled water.
2, the powder pre-treatment processed of bacteria cellulose
The a piece of bacteria cellulose film (8 ± 0.30cm of diameter, thickness 6mm~10mm) prepared is taken to be immersed in a concentration of
In 1% oxalic acid solution.Water-bath is taken to impregnate, temperature is 80 DEG C, 1~2h of time.
3, the drying of bacteria cellulose
The bacteria cellulose film that taking-up was impregnated with oxalic acid solution blots surface moisture with filter paper, is placed in 105 DEG C of electricity of preheating
Middle drying is to constant weight in hot constant temperature blast drying oven.
4, the preparation of bacteria cellulose powder
Dry bacteria cellulose film is taken out, is put in bowl and is ground into powder.
5, the removal of oxalic acid
Bacteria cellulose powder is placed in 100mL beakers, point 2~3 addition absolute ethyl alcohol washings, residual ethanol is natural
Volatilization.
Embodiment 3
1, the preparation and purification of bacteria cellulose
Corn gluten water culture medium is left to ferment and obtains after bacteria cellulose film is optimized by laboratory, and standing for fermentation is specific
For 28~32 DEG C of temperature, time：6~10 days.
The purifying of BC：The BC film distilled water flushings for taking out fermentation are multiple, after surface impurity is removed, then immerse
In the NaOH solution of 0.1mol/L, boil 2h to remove remaining thalline and culture medium, until film be creamy white it is translucent.Afterwards
It is rinsed repeatedly to neutrality, is immersed stored refrigerated for use in distilled water with a concentration of 1% acetic acid and distilled water.
2, the powder pre-treatment processed of bacteria cellulose
The a piece of bacteria cellulose film (8 ± 0.30cm of diameter, thickness 6mm~10mm) prepared is taken to be immersed in a concentration of
In 10% oxalic acid solution.It is 50 DEG C to take ultrasonic wave assistant soakage, power 90W, temperature, time 30min.
3, the drying of bacteria cellulose
The bacteria cellulose film that taking-up was impregnated with oxalic acid solution blots surface moisture with filter paper, is placed in 105 DEG C of electricity of preheating
Middle drying is to constant weight in hot constant temperature blast drying oven.
4, the preparation of bacteria cellulose powder
Dry bacteria cellulose film is taken out, is put in bowl and is ground into powder.
5, the removal of oxalic acid
Bacteria cellulose powder is placed in 100mL beakers, point 2~3 addition absolute ethyl alcohol washings, residual ethanol is natural
Volatilization.
Embodiment 4
1, the preparation and purification of bacteria cellulose
Corn gluten water culture medium is left to ferment and obtains after bacteria cellulose film is optimized by laboratory, and standing for fermentation is specific
For 28~32 DEG C of temperature, time：6~10 days.
The purifying of BC：The BC film distilled water flushings for taking out fermentation are multiple, after surface impurity is removed, then immerse
In the NaOH solution of 0.1mol/L, boil 2h to remove remaining thalline and culture medium, until film be creamy white it is translucent.Afterwards
It is rinsed repeatedly to neutrality, is immersed stored refrigerated for use in distilled water with a concentration of 1% acetic acid and distilled water.
2, the powder pre-treatment processed of bacteria cellulose
The a piece of bacteria cellulose film (8 ± 0.30cm of diameter, thickness 6mm~10mm) prepared is taken to be immersed in a concentration of
In 15% oxalic acid solution.Water-bath is taken to impregnate, temperature is 90 DEG C, 1~2h of time.
3, the drying of bacteria cellulose
The bacteria cellulose film that taking-up was impregnated with oxalic acid solution blots surface moisture with filter paper, is placed in 105 DEG C of electricity of preheating
Middle drying is to constant weight in hot constant temperature blast drying oven.
4, the preparation of bacteria cellulose powder
Dry bacteria cellulose film is taken out, is put in bowl and is ground into powder.
5, the removal of oxalic acid
Bacteria cellulose powder is placed in 100mL beakers, point 2~3 addition absolute ethyl alcohol washings, residual ethanol is natural
Volatilization.
Embodiment 5
1, the preparation and purification of bacteria cellulose
Corn gluten water culture medium is left to ferment and obtains after bacteria cellulose film is optimized by laboratory, and standing for fermentation is specific
For 28~32 DEG C of temperature, time：6~10 days.
The purifying of BC：The BC film distilled water flushings for taking out fermentation are multiple, after surface impurity is removed, then immerse
In the NaOH solution of 0.1mol/L, boil 2h to remove remaining thalline and culture medium, until film be creamy white it is translucent.Afterwards
It is rinsed repeatedly to neutrality, is immersed stored refrigerated for use in distilled water with a concentration of 1% acetic acid and distilled water.
2, the powder pre-treatment processed of bacteria cellulose
(1) a piece of bacteria cellulose film (8 ± 0.30cm of diameter, thickness 6mm~10mm) prepared is taken to be immersed in concentration
For in 5% oxalic acid solution.It is 60 DEG C to take ultrasonic wave assistant soakage, power 90W, temperature, time 20min.
3, the drying of bacteria cellulose
The bacteria cellulose film that taking-up was impregnated with oxalic acid solution blots surface moisture with filter paper, is placed in 105 DEG C of electricity of preheating
Middle drying is to constant weight in hot constant temperature blast drying oven.
4, the preparation of bacteria cellulose powder
Dry bacteria cellulose film is taken out, is put in bowl and is ground into powder.
5, the removal of oxalic acid
Bacteria cellulose powder is placed in 100mL beakers, point 2~3 addition absolute ethyl alcohol washings, residual ethanol is natural
Volatilization.
Claims (10)
1. a kind of preparation method of high-crystallinity bacteria cellulose powder, it is characterised in that：Bacteria cellulose film is impregnated first
In the oxalic acid solution that mass percent concentration is 1%~20%, bacteria cellulose film is then taken out, its surface moisture is blotted,
Then it is dried to constant weight, is finally ground to powdered, acquisition bacteria cellulose powder.
2. wanting a kind of preparation method of high-crystallinity bacteria cellulose powder described in 1 according to right, it is characterised in that：By bacterium
After cellulose is immersed in oxalic acid solution, impregnated using ultrasonic wave assistant soakage or water-bath.
3. wanting a kind of preparation method of high-crystallinity bacteria cellulose powder described in 2 according to right, it is characterised in that：Using super
The condition of sound wave assistant soakage is：90~100W of power, temperature are 50~60 DEG C, and the time is 15~30min；It is impregnated using water-bath
Condition be：Temperature is 80~90 DEG C, 1~2h of time.
4. wanting a kind of preparation method of high-crystallinity bacteria cellulose powder described in 1 according to right, it is characterised in that：Described
Bacteria cellulose film is so that corn gluten water culture medium is left to ferment and is obtained, and standing for fermentation is specially 28~32 DEG C of temperature, time：
6~10 days.
5. wanting a kind of preparation method of high-crystallinity bacteria cellulose powder described in 4 according to right, it is characterised in that：Described
Corn gluten water culture medium ingredient is：Maize pulp-water thinner ratio 1:(1~5), sucrose：33.2g/L calcium chloride：23g/L,
KH2PO4：1.2g/L, MgSO4：0.5g/L, ethyl alcohol：16.2ml/L, the culture medium are acid solution.
6. wanting a kind of preparation method of high-crystallinity bacteria cellulose powder described in 4 according to right, it is characterised in that：Described
Bacteria cellulose film is immersed in alkaline solution first before being immersed in oxalic acid solution, is boiled to remove remaining bacterium
Body and culture medium, until bacteria cellulose film be creamy white it is translucent.
7. wanting a kind of preparation method of high-crystallinity bacteria cellulose powder described in 6 according to right, it is characterised in that：Described
Bacteria cellulose film removes surface impurity first, is then immersed in removal residual thalline and culture medium in alkaline solution again, finally
Multiple flushing is neutrality up to solution, is finally immersed in distilled water and refrigerates.
8. wanting a kind of preparation method of high-crystallinity bacteria cellulose powder described in 1 or 4 according to right, it is characterised in that：Institute
The bacteria cellulose film a diameter of 8 ± 0.30cm, thickness 6mm~10mm stated.
9. wanting a kind of preparation method of high-crystallinity bacteria cellulose powder described in 1 according to right, it is characterised in that：It is described thin
Fungin film is ground to be washed 2~3 times for absolute ethyl alcohol after powder, is added, and residual ethanol is volatilized naturally.
10. a kind of preparation method of high-crystallinity bacteria cellulose powder, it is characterised in that：Include the following steps：
(1) preparation and purification of bacteria cellulose
Bacteria cellulose film is with corn gluten water culture medium is left to ferment and is obtained, wherein medium pH 5, corn gluten and water
Thinner ratio be 1:4, sucrose：33.2g/L calcium chloride：23g/L, KH2PO4：1.2g/L, MgSO4：0.5g/L, ethyl alcohol 16.2ml/
L；
After the bacteria cellulose film removal surface impurity after fermentation, it is immersed in lye and boils, remove remaining thalline and training
Support base, until bacteria cellulose film be creamy white it is translucent；Then use dilute acetic acid solution and distilled water flushing to neutrality；
(2) the powder pre-treatment processed of bacteria cellulose
The bacteria cellulose film that step (1) obtains is immersed in oxalic acid solution, is impregnated using ultrasonic wave assistant soakage or water-bath；
(3) drying of bacteria cellulose
The bacteria cellulose film that step (2) is obtained blots surface moisture, dry to constant weight；
(4) preparation of bacteria cellulose powder
The bacteria cellulose that step (3) obtains is ground into powder；
(5) removal of oxalic acid
The bacteria cellulose powder that step (4) obtains is washed 2~3 times with absolute ethyl alcohol, residual ethanol is volatilized naturally.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110194446A (en) * | 2019-06-10 | 2019-09-03 | 广西科学院 | A kind of 2D cellulose obtained using cellulose depth hydrolysis is the graphene 2D raw powder's production technology of raw material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102694139A (en) * | 2012-05-18 | 2012-09-26 | 东华大学 | Bacterial cellulose-Nafion sandwich proton exchange membrane and preparation and application thereof |
| CN104525148A (en) * | 2015-01-12 | 2015-04-22 | 国家电网公司 | Method for preparing ammonium sulfamate bacterial celluloses for absorbing Pb2+ in waste water |
| CN107201392A (en) * | 2017-05-31 | 2017-09-26 | 陕西科技大学 | A kind of method of cornstarch yellow wastewater processing |
-
2018
- 2018-05-30 CN CN201810540772.2A patent/CN108395562B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102694139A (en) * | 2012-05-18 | 2012-09-26 | 东华大学 | Bacterial cellulose-Nafion sandwich proton exchange membrane and preparation and application thereof |
| CN104525148A (en) * | 2015-01-12 | 2015-04-22 | 国家电网公司 | Method for preparing ammonium sulfamate bacterial celluloses for absorbing Pb2+ in waste water |
| CN107201392A (en) * | 2017-05-31 | 2017-09-26 | 陕西科技大学 | A kind of method of cornstarch yellow wastewater processing |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110194446A (en) * | 2019-06-10 | 2019-09-03 | 广西科学院 | A kind of 2D cellulose obtained using cellulose depth hydrolysis is the graphene 2D raw powder's production technology of raw material |
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